| 摘要: |
| 建立了牛奶中粘菌素和杆菌肽药物残留的固相萃取-超高效液相色谱-串联质谱测定方法，样品用4%三氯乙酸乙腈提取，经乙醚脱脂，过HLB固相萃取柱净化，供液相色谱-串联质谱法分析，外标法定量。结果表明：粘菌素和杆菌肽标准溶液在20～2000 ?g/L范围内呈现良好线性，r2均大于0.998；方法检出限为5 礸/kg，定量限为10 礸/kg；粘菌素和杆菌肽分别在10～100 礸/kg和10～1000 礸/kg添加范围内的平均回收率为84%～110%，批内、批间RSD均小于20%。该方法具有简便快捷、灵敏度高、定性准确等优点，能满足食品安全检测有关法规的要求。 |
| 关键词: 固相萃取 超高效液相色谱-串联质谱 粘菌素、杆菌肽 残留 牛奶 |
| DOI： |
| 投稿时间：2011-06-01修订日期：2011-06-01 |
| 基金项目:国家科技支撑计划课题资助项目（2006BAD31B09） |
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| Determination of Colistin and Bacitracin Residues in Milk by SPE- UPLC-MS/MS |
| liuqi |
| (China institute of veterinary drug control) |
| Abstract: |
| A ultral performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for the simultaneous determination of colistin and bacitracin residues in milk. The samples were extracted by 4% TCA acetonitril, cleaned up with HLB solid phase extraction (SPE) column. The separation and identify of colistin and bacitracin was performed on UPLC-MS/MS. The method was quantified by external standard method. The calibration curves were linear between the peak areas and the concentrations of 20～2000 ?g/L with correlation coefficients(r2)more than 0.998. The limit of detection of colistin and bacitracin were all 5 μg/kg, and the limit of quantitation were 10 μg/kg. The average recoveries from spiked milk at concentrations of 10～50 礸/kg and 10～500 礸/kg ranged from 81% to 116% and the relative standard deviations of intra- and inter-batch were both less than 20% |
| Key words: SPE UPLC-MS/MS Colistin Bacitracin residues milk |
